CN107082816A - A kind of pomace selective oxidation cellulose derivative and preparation method thereof - Google Patents

A kind of pomace selective oxidation cellulose derivative and preparation method thereof Download PDF

Info

Publication number
CN107082816A
CN107082816A CN201710335528.8A CN201710335528A CN107082816A CN 107082816 A CN107082816 A CN 107082816A CN 201710335528 A CN201710335528 A CN 201710335528A CN 107082816 A CN107082816 A CN 107082816A
Authority
CN
China
Prior art keywords
pomace
selective oxidation
preparation
cellulose
cellulose derivative
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710335528.8A
Other languages
Chinese (zh)
Other versions
CN107082816B (en
Inventor
陈雪峰
李列琴
刘宁
房斐
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201710335528.8A priority Critical patent/CN107082816B/en
Publication of CN107082816A publication Critical patent/CN107082816A/en
Application granted granted Critical
Publication of CN107082816B publication Critical patent/CN107082816B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/02Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C5/00Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The invention discloses a kind of pomace selective oxidation cellulose derivative and preparation method thereof, comprise the following steps:1) 1g is pressed:(10~35) mL solid-liquid ratio, sodium periodate solution is added into pomace cellulose, at 30~50 DEG C, and constant temperature oscillation reacts 2~10h, collected by suction filter residue;2) filter residue is soaked into 0.3~1h with 0.1~0.2mol/L ethylene glycol solution, then uses water cyclic washing, suction filtration dries filter residue to constant weight, and pomace selective oxidation cellulose derivative is made.The present invention is from sodium metaperiodate as oxidant, and oxidation effectiveness is good, and reaction condition and the extent of reaction are easily controlled, and product is easy to real-time detection, is conducive to expanding economical utilizing about apple scope, suitable for industrialized production.

Description

A kind of pomace selective oxidation cellulose derivative and preparation method thereof
Technical field
The invention belongs to food processing technology field, and in particular to a kind of pomace selective oxidation fiber simple and easy to apply Plain derivative and preparation method thereof.
Background technology
China is apple production big country, is shown according to relevant statistics, and national apple production total amount in 2016 is up to 43,800,000 Ton, especially in the apple production base using Shaanxi Province as representative, apple production is up to nearly 10,000,000 tons.Along with apple production Increase, apple processing industry grows stronger day by day, and this is made that huge contribution for China's economic development to a certain extent, and with This simultaneously, the leftover bits and pieces produced in its process --- pomace more rationally using then turn into one be badly in need of solve ask Topic.
Research shows, containing a variety of nutriments such as dietary fiber, mineral matters in pomace, and value is high, wherein meals Food fiber is up to 60~80%, and the class important substance in dietary cellulosic is exactly cellulose, and its content accounts for pomace meals Eat 60% or so of fiber.Though cellulose can not be decomposed with utilizing by human body, have in terms of human gastrointestinal tract digestion is adjusted Important effect.It can adsorb large quantity of moisture, increase excrement amount, promote enterocinesia, accelerate the excretion of excrement, carcinogen is existed Shorter residence time in enteron aisle, reduces the pessimal stimulation to enteron aisle and acts on, so as to prevent intestinal cancer.It is fine from structure Dimension element be it is a kind of by glucose group into macromolecular polysaccharide, each other with β-Isosorbide-5-Nitrae glycosidic bond links between each glucose unit, by There is hydrogen bond in intermolecular, thus it is more stable under normal temperature, and be not easily decomposed.From the point of view of physical property, cellulose is water insoluble With general organic solvent, there is certain difficulty so using.
In recent years, researcher has found that oxidation is the hydroxyl quilt on a kind of effective cellulose modified method, glucose molecule Aldehyde radical or carboxyl are oxidized to, its retentiveness, dispersiveness etc. can be increased.The method of cellulose oxidation is varied, common are NaIO4Oxidation system method, NaClO/TEMPO/NaBr oxidation systems method, NHPI/ anthraquinone oxidation system methods etc..Many celluloses Oxidation technology shows that general oxidant can make the hydroxyl on cellulose each unit carbon atom produce random oxidation, simultaneously Aldehyde radical, carboxyl, ketone etc. are produced, causes oxidation system more complicated, research is not easy to.
Li Yong (research of cellulose selective oxidation, 2014) uses TCCA/TEMPO/NaBr oxidation systems, have studied fibre Oxidation of the plain powder of dimension in acetone-water combination solvent, as a result shows, this system can be by the primary hydroxyl on cellulosic structure unit Based selective is oxidized to carboxyl, and reaction rate is very fast.But the oxidant sym-closene (TCCA) that this method is used is in height Temperature is lower easily to decompose, can give off poisonous gas, unstable.
Wear (preparation of TEMPO oxidizing process nano-cellulose and its composite membrane and performance study, 2015) of heap of stone and use NaClO/ Selective oxidation cellulose primary hydroxyl group generates carboxylic group to TEMPO/NaBr systems in aqueous, is prepared for oxidation nanometer fine Dimension element.But the reaction can only control cellulose oxidation in the stage of generation carboxyl, its intelligent control and reaction efficiency need Lifting.
The content of the invention
In view of the above-mentioned drawbacks of the prior art, fine it is an object of the invention to provide a kind of pomace selective oxidation Plain derivative of dimension and preparation method thereof, this method is simple to operate, and course of reaction is stable, safety, is easy to control and studies;Through the party Pomace selective oxidation cellulose derivative made from method has higher water retention property.
The present invention is to be achieved through the following technical solutions:
The invention discloses a kind of preparation method of pomace selective oxidation cellulose derivative, comprise the following steps:
1) 1g is pressed:(10~35) mL solid-liquid ratio, sodium periodate solution is added into pomace cellulose, at 30~50 DEG C Under, constant temperature oscillation reacts 2~10h, collected by suction filter residue;
2) filter residue is soaked into 0.3~1h with 0.1~0.2mol/L ethylene glycol solution, then uses water cyclic washing, suction filtration will Filter residue is dried to constant weight, and pomace selective oxidation cellulose derivative is made.
Step 1) described in sodium periodate solution concentration be 0.2~0.6mol/L.
Step 1) it is that constant temperature oscillation reaction is carried out with 120~160r/min rotating speed.
Step 2) it is described drying be at 40~60 DEG C carry out.
Preferably, the pomace cellulose is made by following steps:
(1) water, glacial acetic acid and sodium chlorite are added into apple insoluble diedairy fiber residue, at 55~75 DEG C, with 28~32kHZ 10~15min of frequency ultrasonic wave vibration processing;
(2) handled to step (1) in obtained product and add glacial acetic acid and sodium chlorite again, at 55~75 DEG C, with 28~32kHZ frequency ultrasonic wave 10~15min of vibration processing, after obtained product is washed with distilled water and acetone successively, Suction filtration, filter residue is dried to constant weight, and the cellulose composite for removing lignin is made;
(3) sodium hydroxide solution is added into the cellulose composite for removing lignin, constant temperature oscillation reacts 10~30h, Product is washed to neutrality, suction filtration, and filter residue is dried to constant weight;
(4) into step (3) products therefrom, sodium hydroxide solution is added, constant temperature oscillation reacts 10~30h, product washing To neutrality, suction filtration, filter residue is dried to constant weight, and pomace cellulose is made.
In step (1), the solid-liquid ratio of apple insoluble diedairy fiber residue and water is 1g:(10~15) mL;Apple is insoluble Property dietary fiber residue and glacial acetic acid amount ratio be 10g:(1~5) mL;Apple insoluble diedairy fiber residue and sodium chlorite Mass ratio be 10:(1~8);
In step (2), glacial acetic acid is identical with step (1) with the addition of sodium chlorite.
In step (3) and (4), the solid-liquid ratio of the cellulose composite and sodium hydroxide solution that remove lignin is 1g:(10 ~25) mL.
In step (3) and (4), the mass concentration of sodium hydroxide solution is 12%~16%.
In step (3) and (4), constant temperature oscillation reaction is entered under conditions of 30~50 DEG C, rotating speed are 120~160r/min OK;Drying is carried out at 40~60 DEG C in step (2), (3) and (4)
The invention also discloses using pomace selective oxidation cellulose derivative made from above-mentioned preparation method.
Compared with prior art, the present invention has following beneficial technique effect:
The preparation method of pomace selective oxidation cellulose derivative disclosed by the invention, oxygen is used as using periodic acid solution Agent, the primary hydroxyl optionally aoxidized on pomace cellulosic structure unit is dialdehyde base, is prepared for pomace selectivity fine The plain oxidized derivatives of dimension.The advantage of the present invention is fairly obvious:First, the inventive method selects sodium metaperiodate as oxidising agent, The reagent is soluble in water, and collocation method is equal to the collocation method of general reagent, simple to operate;And the reagent is selected for cellulose The intelligent control of selecting property oxidation is stronger, can be by cellulose oxidation control in the aldehyde radical stage, and the oxidation product of generation is with higher Retentiveness.Secondly, water-bath is replaced using isothermal vibration in course of reaction, that is, ensure that the continuation of course of reaction, can be avoided again The uneven equal error of stirring artificially caused, it is ensured that the preciseness and high efficiency of course of reaction.Finally, the reaction is easy in real time Testing result, it is ageing good, there is important theory support meaning to being applied to industrial production in the future.
It is double aldocelluloses, reaction system through pomace selective oxidation cellulose derivative made from the inventive method It is clear, it is easy to control and studies;And product has higher retentiveness, it is expected to be applied to field of food preservation in the future.
Further, pomace cellulose used in the present invention, is removed using ultrasonic assistant sodium chlorite method first The lignin of pomace insoluble diedairy fiber, secondly extracts cellulose in the basic conditions, and carries out under identical conditions two Secondary to extract, now pomace cellulose purity can reach 83.02%, and second extraction ensure that the purity of raw material, it is ensured that oxygen Change the authenticity of raw material, and extraction step is simple and easy to apply, is easy to industrial operation.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and It is not to limit.
Embodiment 1
A kind of preparation method of pomace selective oxidation cellulose derivative, comprises the following steps:
1) the apple insoluble diedairy fiber residue of certain mass is weighed, using solid-liquid ratio as 1:10 (g/mL) ratio is added Distilled water, respectively with 10:1 (g/mL) and 10:2 (g/g) ratio adds glacial acetic acid and sodium chlorite, in 28kHZ at 55 DEG C Frequency ultrasonic wave vibrates 10min;
2) to step 1) glacial acetic acid and sodium chlorite are added again in the obtained product of processing, at 55 DEG C, with 28kHZ's Frequency ultrasonic wave vibration processing 10min, obtained product is washed for several times respectively with distilled water and acetone again, suction filtration, filter residue in 40 DEG C of drying as remove the cellulose composite of lignin to constant weight;
3) the appropriate cellulose composite for removing lignin is weighed, using solid-liquid ratio as 1:10 (g/mL) ratio adds concentration For 12% sodium hydroxide solution, it is put into isothermal vibration device with 120r/min rotating speed in reacting 10h at 30 DEG C, distills washing To neutral, suction filtration, filter residue is in 40 DEG C of drying to constant weight;
4) to step 3) product in, using solid-liquid ratio as 1:10 (g/mL) ratio adds the sodium hydroxide that concentration is 12% Solution, is put into isothermal vibration device with 120r/min rotating speed in reacting 10h at 30 DEG C, distills and be washed to neutrality, suction filtration, filter residue In 40 DEG C of drying to constant weight, the dried powder of gained is pomace cellulose;
5) appropriate pomace cellulose is weighed, using solid-liquid ratio as 1:25 (g/mL) ratio adds 0.5mol/L high iodine Acid sodium solution, is put into isothermal vibration device with 160r/min rotating speed in reacting 2h at 45 DEG C, suction filtration, and with 0.1mol/L second Glycol solution soaks 0.3h, then uses distilled water cyclic washing, and suction filtration, filter residue is selected in 40 DEG C of drying to constant weight, as pomace Property oxycellulose derivative.
Apple insoluble diedairy fiber residue used in the embodiment of the present invention, specific preparation method is as follows:
A certain amount of pomace is accurately weighed, is 1 by solid-liquid ratio:25(g:ML ratio) adds distilled water, after stirring 100min is extracted in 70 DEG C, suction filtration stays filter residue, and 60 DEG C of dryings obtain removing the drying filter residue of water-soluble polysaccharide;Removal is weighed again The drying filter residue of water-soluble polysaccharide, is 1 by solid-liquid ratio:20(g:ML) the sodium hydroxide solution of addition 4%, and at 45 DEG C, it is permanent Tepidarium 90min, suction filtration stays filter residue;Add and same amount of 2% hydrochloric acid solution of sodium hydroxide, and at 60 DEG C, thermostatted water 90min is bathed, suction filtration stays filter residue;Filter residue is respectively washed 2 times with absolute ethyl alcohol, acetone, suction filtration, 60 DEG C of drying, that is, obtains apple insoluble Property dietary fiber residue.
Note:Used apple insoluble diedairy fiber residue prepares same the method in following examples, in addition, on Apple insoluble diedairy fiber residue is prepared as this area conventional technical means, therefore is not excluded for other and can prepare apple not The method of soluble dietary fiber residue is used for the present invention.
Embodiment 2
A kind of preparation method of pomace selective oxidation cellulose derivative, comprises the following steps:
1) the apple insoluble diedairy fiber residue of certain mass is weighed, using solid-liquid ratio as 1:12 (g/mL) ratio is added Distilled water, respectively with 10:2 (g/mL) and 10:3 (g/g) ratio adds glacial acetic acid and sodium chlorite, in 30kHZ at 60 DEG C Frequency ultrasonic wave vibrates 12min;
2) to step 1) glacial acetic acid and sodium chlorite are added again in the obtained product of processing, at 60 DEG C, with 30kHZ's Frequency ultrasonic wave vibration processing 12min, obtained product is washed for several times respectively with distilled water and acetone again, suction filtration, filter residue in 45 DEG C of drying as remove the cellulose composite of lignin to constant weight;
3) the appropriate cellulose composite for removing lignin is weighed, using solid-liquid ratio as 1:15 (g/mL) ratio adds concentration For 13% sodium hydroxide solution, it is put into isothermal vibration device with 130r/min rotating speed in reacting 15h at 35 DEG C, distills washing To neutral, suction filtration, filter residue is in 45 DEG C of drying to constant weight;
4) to step 3) product in, using solid-liquid ratio as 1:15 (g/mL) ratio adds the sodium hydroxide that concentration is 13% Solution, is put into isothermal vibration device with 130r/min rotating speed in reacting 15h at 35 DEG C, distills and be washed to neutrality, suction filtration, filter residue In 45 DEG C of drying to constant weight, the dried powder of gained is pomace cellulose;
5) appropriate pomace cellulose is weighed, using solid-liquid ratio as 1:20 (g/mL) ratio adds 0.6mol/L high iodine Acid sodium solution, is put into isothermal vibration device with 150r/min rotating speed in reacting 2h at 40 DEG C, suction filtration, and with 0.15mol/L's Ethylene glycol solution soaks 0.4h, then uses distilled water cyclic washing, and suction filtration, filter residue is selected in 45 DEG C of drying to constant weight, as pomace Selecting property oxycellulose derivative.
Embodiment 3
A kind of preparation method of pomace selective oxidation cellulose derivative, comprises the following steps:
1) the apple insoluble diedairy fiber residue of certain mass is weighed, using solid-liquid ratio as 1:13 (g/mL) ratio is added Distilled water, respectively with 10:3 (g/mL) and 10:4 (g/g) ratio adds glacial acetic acid and sodium chlorite, in 31kHZ at 65 DEG C Frequency ultrasonic wave vibrates 14min;
2) to step 1) glacial acetic acid and sodium chlorite are added again in the obtained product of processing, at 65 DEG C, with 31kHZ's Frequency ultrasonic wave vibration processing 14min, obtained product is washed for several times respectively with distilled water and acetone again, suction filtration, filter residue in 50 DEG C of drying as remove the cellulose composite of lignin to constant weight;
3) the appropriate cellulose composite for removing lignin is weighed, using solid-liquid ratio as 1:20 (g/mL) ratio adds concentration For 14% sodium hydroxide solution, it is put into isothermal vibration device with 140r/min rotating speed in reacting 20h at 40 DEG C, distills washing To neutral, suction filtration, filter residue is in 50 DEG C of drying to constant weight;
4) to step 3) product in, using solid-liquid ratio as 1:20 (g/mL) ratio adds the sodium hydroxide that concentration is 14% Solution, is put into isothermal vibration device with 140r/min rotating speed in reacting 20h at 40 DEG C, distills and be washed to neutrality, suction filtration, filter residue In 50 DEG C of drying to constant weight, the dried powder of gained is pomace cellulose;
5) appropriate pomace cellulose is weighed, using solid-liquid ratio as 1:15 (g/mL) ratio adds 0.6mol/L high iodine Acid sodium solution, is put into isothermal vibration device with 120r/min rotating speed in reacting 6h at 45 DEG C, suction filtration, and with 0.15mol/L's Ethylene glycol solution soaks 0.5h, then uses distilled water cyclic washing, and suction filtration, filter residue is selected in 50 DEG C of drying to constant weight, as pomace Selecting property oxycellulose derivative.
Embodiment 4
A kind of preparation method of pomace selective oxidation cellulose derivative, comprises the following steps:
1) the apple insoluble diedairy fiber residue of certain mass is weighed, using solid-liquid ratio as 1:15 (g/mL) ratio is added Distilled water, respectively with 10:5 (g/mL) and 10:6 (g/g) ratio adds glacial acetic acid and sodium chlorite, in 32kHZ at 75 DEG C Frequency ultrasonic wave vibrates 15min;
2) to step 1) glacial acetic acid and sodium chlorite are added again in the obtained product of processing, at 75 DEG C, with 32kHZ's Frequency ultrasonic wave vibration processing 15min, obtained product is washed for several times respectively with distilled water and acetone again, suction filtration, filter residue in 60 DEG C of drying as remove the cellulose composite of lignin to constant weight;
3) the appropriate cellulose composite for removing lignin is weighed, using solid-liquid ratio as 1:25 (g/mL) ratio adds concentration For 16% sodium hydroxide solution, it is put into isothermal vibration device with 160r/min rotating speed in reacting 25h at 45 DEG C, distills washing To neutral, suction filtration, filter residue is in 60 DEG C of drying to constant weight;
4) to step 3) product in, using solid-liquid ratio as 1:25 (g/mL) ratio adds the sodium hydroxide that concentration is 16% Solution, is put into isothermal vibration device with 160r/min rotating speed in reacting 25h at 45 DEG C, distills and be washed to neutrality, suction filtration, filter residue In 60 DEG C of drying to constant weight, the dried powder of gained is pomace cellulose;
5) appropriate pomace cellulose is weighed, using solid-liquid ratio as 1:25 (g/mL) ratio adds 0.6mol/L high iodine Acid sodium solution, is put into isothermal vibration device with 140r/min rotating speed in reacting 4h at 35 DEG C, suction filtration, and with 0.2mol/L second Glycol solution soaks 0.6h, then uses distilled water cyclic washing, and suction filtration, filter residue is selected in 60 DEG C of drying to constant weight, as pomace Property oxycellulose derivative.
Retentiveness is tested
The present invention determines the retentiveness of the plain oxidized derivatives of pomace selective fiber, i.e., fine primarily directed to pomace Oxycellulose in dimension element and embodiment 1~4 has carried out retentiveness contrast.
Specific method is:0.5g samples accurately are weighed, are put into the centrifuge tube after weighing, 75mL water is added, shakes up, and in 24h is placed at 25 DEG C, 15min is then centrifuged with 4000r/min rotating speed, incline supernatant liquor, uses filter paper suck dry moisture, is claimed Weight.
Sample retentiveness calculation formula is:Retentiveness (g/g)=【(g)-sample dry weight (g) during sample is wet】/ sample dry weight (g)。
Specific experimental result is as shown in table 1.
The cellulose of table 1 and oxycellulose retentiveness measurement result
Sample Cellulose The product of embodiment 1 The product of embodiment 2 The product of embodiment 3 The product of embodiment 4
Retentiveness (g/g) 3.44 5.60 5.78 6.51 6.07
As shown in Table 1, under the conditions of same measured, the retentiveness of oxycellulose is apparently higher than cellulose, and this explanation is fine The selective oxidation of dimension element can significantly improve its retentiveness, and reason is the c-c of 2,3 on cellulose glucose unit after oxidation Key is broken, and has increased hydrophilic couple of aldehyde functions newly, and crystallinity is reduced, and structure is looser, causes the parent of hydrophilic radical Outlet capacity is strengthened.Accordingly, the pomace selective oxidation cellulose derivative prepared by the present invention would be possible to turn into food A kind of new material or intermediate raw material of product preservation field, reliable technical support is provided for the development of food service industry in future.
In summary, the present invention removes pomace insoluble diedairy fiber using ultrasonic assistant sodium chlorite method first Lignin;Secondly cellulose is extracted in the basic conditions, and carry out under identical conditions second extraction, now pomace cellulose Purity reaches 83.02%;Then using this cellulose as raw material, sodium metaperiodate carries out the oxidation experiment of cellulose as oxidant, The plain oxidized derivatives of the pomace selective fiber with higher retentiveness are made.

Claims (10)

1. a kind of preparation method of pomace selective oxidation cellulose derivative, it is characterised in that comprise the following steps:
1) 1g is pressed:(10~35) mL solid-liquid ratio, sodium periodate solution is added into pomace cellulose, at 30~50 DEG C, Constant temperature oscillation reacts 2~10h, collected by suction filter residue;
2) filter residue is soaked into 0.3~1h with 0.1~0.2mol/L ethylene glycol solution, then uses water cyclic washing, suction filtration, by filter residue Pomace selective oxidation cellulose derivative is made to constant weight in drying.
2. the preparation method of pomace selective oxidation cellulose derivative according to claim 1, it is characterised in that step It is rapid 1) described in sodium periodate solution concentration be 0.2~0.6mol/L.
3. the preparation method of pomace selective oxidation cellulose derivative according to claim 1, it is characterised in that step 1) rapid be to carry out constant temperature oscillation reaction with 120~160r/min rotating speed.
4. the preparation method of pomace selective oxidation cellulose derivative according to claim 1, it is characterised in that step Rapid 2) described drying is carried out at 40~60 DEG C.
5. the preparation method of the pomace selective oxidation cellulose derivative according to any one in Claims 1 to 4, Characterized in that, the pomace cellulose is made by following steps:
(1) water, glacial acetic acid and sodium chlorite are added into apple insoluble diedairy fiber residue, at 55~75 DEG C, with 28~ 32kHZ 10~15min of frequency ultrasonic wave vibration processing;
(2) handled to step (1) in obtained product and add glacial acetic acid and sodium chlorite again, at 55~75 DEG C, with 28~ 32kHZ frequency ultrasonic wave 10~15min of vibration processing, after obtained product is washed with distilled water and acetone successively, suction filtration, Filter residue is dried to constant weight, and the cellulose composite for removing lignin is made;
(3) sodium hydroxide solution is added into the cellulose composite for removing lignin, constant temperature oscillation reacts 10~30h, product Neutrality, suction filtration are washed to, filter residue is dried to constant weight;
(4) into step (3) products therefrom, sodium hydroxide solution is added, constant temperature oscillation reacts 10~30h, during product is washed to Property, suction filtration, filter residue dried to constant weight, and pomace cellulose is made.
6. the preparation method of pomace selective oxidation cellulose derivative according to claim 5, it is characterised in that step Suddenly in (1), the solid-liquid ratio of apple insoluble diedairy fiber residue and water is 1g:(10~15) mL;Apple insoluble diedairy fiber The amount ratio of residue and glacial acetic acid is 10g:(1~5) mL;The mass ratio of apple insoluble diedairy fiber residue and sodium chlorite is 10:(1~8);
In step (2), glacial acetic acid is identical with step (1) with the addition of sodium chlorite.
7. the preparation method of pomace selective oxidation cellulose derivative according to claim 5, it is characterised in that step Suddenly in (3) and (4), the solid-liquid ratio of the cellulose composite and sodium hydroxide solution that remove lignin is 1g:(10~25) mL.
8. the preparation method of pomace selective oxidation cellulose derivative according to claim 5, it is characterised in that step Suddenly in (3) and (4), the mass concentration of sodium hydroxide solution is 12%~16%.
9. the preparation method of pomace selective oxidation cellulose derivative according to claim 5, it is characterised in that step Suddenly in (3) and (4), constant temperature oscillation reaction is carried out under conditions of 30~50 DEG C, rotating speed are 120~160r/min;Step (2), drying is carried out at 40~60 DEG C in (3) and (4).
10. spread out using pomace selective oxidation cellulose made from the preparation method described in any one in claim 1~9 It is biological.
CN201710335528.8A 2017-05-12 2017-05-12 A kind of apple pomace selective oxidation cellulose derivative and preparation method thereof Active CN107082816B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710335528.8A CN107082816B (en) 2017-05-12 2017-05-12 A kind of apple pomace selective oxidation cellulose derivative and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710335528.8A CN107082816B (en) 2017-05-12 2017-05-12 A kind of apple pomace selective oxidation cellulose derivative and preparation method thereof

Publications (2)

Publication Number Publication Date
CN107082816A true CN107082816A (en) 2017-08-22
CN107082816B CN107082816B (en) 2019-11-05

Family

ID=59607439

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710335528.8A Active CN107082816B (en) 2017-05-12 2017-05-12 A kind of apple pomace selective oxidation cellulose derivative and preparation method thereof

Country Status (1)

Country Link
CN (1) CN107082816B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109183506A (en) * 2018-08-31 2019-01-11 王成 A kind of preparation method of drying strengthening agent
CN116277346A (en) * 2023-03-07 2023-06-23 南京林业大学 High-strength transparent wood film and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101367878A (en) * 2008-07-24 2009-02-18 吴茂玉 Method for preparing high-viscosity sodium carboxymethylcellulose with apple residue
WO2014062129A1 (en) * 2012-10-18 2014-04-24 Kth Holding Ab Regioselective modification of a xyloglucan hemicellulose for high-performance biopolymer barrier films
US20150147558A1 (en) * 2012-06-04 2015-05-28 Symatese Oxidized cellulose-based material, method for obtaining same and use thereof as compress
CN105111256A (en) * 2015-08-16 2015-12-02 李玉山 Integrated extracting and purifying method for active ingredients of apple pomace

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101367878A (en) * 2008-07-24 2009-02-18 吴茂玉 Method for preparing high-viscosity sodium carboxymethylcellulose with apple residue
US20150147558A1 (en) * 2012-06-04 2015-05-28 Symatese Oxidized cellulose-based material, method for obtaining same and use thereof as compress
WO2014062129A1 (en) * 2012-10-18 2014-04-24 Kth Holding Ab Regioselective modification of a xyloglucan hemicellulose for high-performance biopolymer barrier films
CN105111256A (en) * 2015-08-16 2015-12-02 李玉山 Integrated extracting and purifying method for active ingredients of apple pomace

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
吴晓杰等: "纤维素选择性氧化制备二醛纤维素", 《辽东学院学报(自然科学版)》 *
李丽等: "苹果渣中纤维素、半纤维素的提取分离", 《食品科技》 *
赵斌等: "利用高碘酸钠氧化制备椰衣醛基纤维", 《天然产物研究与开发》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109183506A (en) * 2018-08-31 2019-01-11 王成 A kind of preparation method of drying strengthening agent
CN116277346A (en) * 2023-03-07 2023-06-23 南京林业大学 High-strength transparent wood film and preparation method thereof
CN116277346B (en) * 2023-03-07 2024-02-06 南京林业大学 High-strength transparent wood film and preparation method thereof

Also Published As

Publication number Publication date
CN107082816B (en) 2019-11-05

Similar Documents

Publication Publication Date Title
CN106146687B (en) A kind of method of pectin in extraction citrus peel residue
CN109232909B (en) Method for separating high-activity lignin from agriculture and forestry biomass
CN102212976B (en) Method for separating bagasse cellulose from lignin
CN107686524B (en) V6- type crystalline texture potato starch-fatty acid complexes preparation method
CN104987428B (en) A kind of complex enzyme microwave extract method of the white thorn polysaccharide of utilization Response Surface Method optimization
CN104086667A (en) Method for preparing pectin from citrus fruit peel residues by employing ultrasonic-assisted extraction
CN107082816B (en) A kind of apple pomace selective oxidation cellulose derivative and preparation method thereof
CN103554274B (en) A kind of preparation method of sugarcane marrow SURGICEL
CN102276760A (en) Method for separating and purifying hemicelluloses from agriculture and forest biomasses by gradient ethanol precipitation
CN103467627A (en) Preparation method for corn stalk hemicellulose
CN110551295A (en) Method for separating chemical components of gramineous plants and purifying lignin
CN108166293B (en) A kind of method and its system of irradiation-plant fibrous agricultural wastes of chemical method Combined Treatment
CN105249481B (en) It is a kind of extracted by mulberry leaf after the residue method of producing high swelling property dietary fiber
CN114045315A (en) Method for improving enzymolysis efficiency of licorice residue
CN106866381B (en) Method for preparing moso bamboo lignin monophenol compound
CN106086084A (en) The preprocess method of a kind of Ethanol Production Process with Straw and application
CN110240709A (en) A method of acidification strengthens tetrahydrofurfuryl alcohol pretreatment and extracts lignin in walnut shell
CN103881115B (en) A kind of method strengthening enzymolysis process extraction tobacco leaf xylogen
CN109170922A (en) A kind of preparation method of wheat bran soluble dietary fiber
CN107987862A (en) The method that a kind of Asia/supercritical methanol liquified cellulosic prepares primary biomass platform chemicals
CN104432110B (en) A kind of preparation method of Sulfation Fructus Mali pumilae water soluble dietary fiber
CN105504075A (en) Method for reducing molecular weight of starch through dry method
CN102733219B (en) Method for extracting cellulose from tobacco waste based on reductant-oxidant
CN106883315A (en) A kind of method that pectin is extracted from kiwifruit peel
CN104432109B (en) The method of Sulfation water-soluble dietary fiber is prepared in a kind of extruding

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant